Toluene purification device in etifolin hydrochloride production

Abstract

The utility model relates to the technical field of chemical production equipment, and discloses a toluene purification device in etifolin hydrochloride production, which comprises a crude toluene storage tank, an evaporator and a first gas-liquid separator which are sequentially communicated through pipelines and valves, the first gas-liquid separator is provided with a light phase discharge port and a heavy phase discharge port, and the light phase discharge port of the first gas-liquid separator is sequentially communicated with a first condenser, a second condenser and a second gas-liquid separator through pipelines and valves; the second gas-liquid separator is provided with a light phase discharge port and a heavy phase discharge port, and the light phase discharge port of the second gas-liquid separator is communicated to the toluene layering tank; toluene outlets in the top of the toluene layering tank are sequentially communicated with the salt tower through pipelines and valves, and toluene outlets in the top of the salt tower are sequentially communicated with the anhydrous toluene storage tank through pipelines and valves. The device is simple in process flow and good in purification effect, the obtained product can be sold as a commodity, and the enterprise benefit is increased.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical production equipment, in particular to a toluene purification device in the production of etilefrine hydrochloride. Background Art

[0002] Etilefrine hydrochloride, chemically known as 2-ethylamino-1-[3-hydroxyphenyl]ethanol hydrochloride and with the molecular formula C10H15NO2·HCl, is a widely used pharmaceutical intermediate. Its functions include strengthening myocardial contractility, constricting blood vessels, and raising blood pressure, primarily for emergency medical treatment of hypotension. The current method for producing etilefrine hydrochloride, which involves the reaction of α-bromo-m-hydroxyacetophenone with N-ethylbenzylamine, ultimately produces etilefrine hydrochloride and toluene. Because the amination reaction typically uses 40-80 wt% ethanol as the solvent, the toluene obtained by distillation after the reaction contains significant amounts of impurities such as water and ethanol, making it unsuitable for commercial sale. Disposing of the toluene as waste would pollute the environment. Therefore, purification is required to ensure compliance with environmental standards for sale to ensure environmental safety and increase business profitability. Summary of the Invention

[0003] The technical problem to be solved by the utility model is to provide a toluene purification device in the production of etilefrine hydrochloride, which has a simple process flow and good purification effect. The obtained product can be sold as a commodity to increase the efficiency of the enterprise.

[0004] In order to solve the above technical problems, the technical solution of the utility model is:

[0005] A toluene purification device for etilefrine hydrochloride production comprises a crude toluene storage tank, an evaporator, and a first gas-liquid separator, which are sequentially connected via pipelines and valves; the first gas-liquid separator is provided with a light phase discharge port and a heavy phase discharge port, and the light phase discharge port of the first gas-liquid separator is sequentially connected to a first condenser, a second condenser, and a second gas-liquid separator via pipelines and valves; the second gas-liquid separator is provided with a light phase discharge port and a heavy phase discharge port, and the light phase discharge port of the second gas-liquid separator is connected to a toluene stratification tank; the toluene outlet at the top of the toluene stratification tank is sequentially connected to a salt tower via pipelines and valves, and the toluene outlet at the top of the salt tower is sequentially connected to an anhydrous toluene storage tank via pipelines and valves.

[0006] Preferably, the evaporator is a rising film evaporator, which is a DN450 shell and tube heat exchanger, manufactured by Zibo Shuangte Chemical Equipment Co., Ltd.

[0007] Preferably, a pipeline thermometer and a steam regulating valve are provided in the pipeline between the evaporator and the first gas-liquid separator. The pipeline thermometer and the steam regulating valve are interlocked to control the distillation temperature. The interlocking control is controlled by a DCS automatic control system.

[0008] Preferably, the discharge port of the first condenser is also connected to an ethanol storage tank through a pipeline.

[0009] Preferably, the first gas-liquid separator is a rising film gas-liquid separator, the second gas-liquid separator is a rising film after-cooling gas-liquid separator, and the first gas-liquid separator and the second gas-liquid separator are both DN400 rising film gas-liquid separators, and the manufacturer is Huludao Bohai Jintai Industrial Co., Ltd.

[0010] Preferably, the first condenser and the second condenser are both spiral plate condensers, the first condenser is a F50 m2 condenser, and the second condenser is a F20 m2 condenser, and the manufacturer of both is Shandong Hunter Industrial Equipment Manufacturing Co., Ltd.

[0011] Preferably, the heavy phase discharge ports of the first gas-liquid separator and the second gas-liquid separator are both connected to impurity storage tanks through pipelines and valves.

[0012] Preferably, the second gas-liquid separator is further provided with a vent pipe. The rising film vent pipe is connected to a toluene removal activated carbon adsorption system to adsorb part of the vaporized toluene.

[0013] Preferably, the water outlet at the bottom of the toluene stratification tank is connected to a water storage tank through a pipeline and a valve.

[0014] Preferably, the pipeline connecting the toluene separation tank to the salt tower and the pipeline connecting the salt tower to the anhydrous toluene storage tank are both equipped with an online automatic moisture detector. The online automatic moisture detector is an SCK106 trace moisture analyzer, manufactured by Shandong Shengkang Electric Co., Ltd. When the online automatic moisture detector detects that the moisture content in the toluene does not meet the salt tower inlet standard (2%-3%), the aqueous toluene is returned to the toluene separation tank for further separation of water and toluene, wherein the separated water is collected in the water storage tank, and the unseparated water is transferred to the salt tower together with the toluene for further separation. If the toluene content output by the salt tower is higher than the set standard, the toluene is returned to the salt tower for further separation.

[0015] Preferably, the brine outlet at the bottom of the salt tower is connected to the brine storage tank in sequence through a pipeline and a valve. The salt tower is a dehydration and drying tower, and the filler is large-grained sodium chloride with a particle size of 10 mm and large-grained calcium chloride with a particle size of 5 mm.

[0016] Due to the adoption of the above technical solution, the beneficial effects of the utility model are:

[0017] The utility model first separates ethanol from crude toluene through an evaporator, and then distills out water and toluene. The remaining part of other impurities (reaction raw materials and products, solvent residues, etc.) are separated from part of the water and other impurities after the water and toluene enter the first gas-liquid separator. Then, the water and other impurities are separated through further condensation and separation through the first condenser, the second condenser, and the second gas-liquid separator. The obtained toluene solution contains only part of water. The water-containing toluene is allowed to stand in a toluene stratification tank for stratification. The water content of the toluene in the upper layer is between 2% and 3%. The toluene is transported to a salt tower for dehydration to obtain toluene with a water content of less than 0.05%, which is higher than the water content of the industrial toluene product standard of less than 1%, and can therefore be sold as a commodity.

[0018] In short, the process flow of the utility model is simple, the purification effect is good, and the obtained product can be sold as a commodity to increase the benefits of the enterprise. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a structural schematic diagram of an embodiment of the utility model;

[0020] In the figure, 1. crude toluene storage tank; 2. evaporator; 3. first gas-liquid separator; 4. first condenser; 5. second condenser; 6. second gas-liquid separator; 7. toluene delamination tank; 8. salt tower; 9. anhydrous toluene storage tank; 10. impurity storage tank; 11. ethanol storage tank; 12. water storage tank; 13. brine storage tank. DETAILED DESCRIPTION

[0021] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0022] Example 1

[0023] like Figure 1 As shown, a toluene purification device in the production of etilefrine hydrochloride includes a crude toluene storage tank 1, an evaporator 2, and a first gas-liquid separator 3, which are connected in sequence through pipes (not marked) and valves (not marked); the first gas-liquid separator 3 is provided with a light phase discharge port (not marked) and a heavy phase discharge port (not marked), and the light phase discharge port of the first gas-liquid separator 3 is connected in sequence to a first condenser 4, a second condenser 5, and a second gas-liquid separator 6 through pipes and valves; the second gas-liquid separator 6 is provided with a light phase discharge port and a heavy phase discharge port, and the light phase discharge port of the second gas-liquid separator 6 is connected to a toluene delamination tank 7; the toluene outlet at the top of the toluene delamination tank 7 is connected in sequence to a salt tower 8 through pipes and valves, and the toluene outlet at the top of the salt tower 8 is connected in sequence to an anhydrous toluene storage tank 9 through pipes and valves.

[0024] The heavy phase discharge ports of the first gas-liquid separator 3 and the second gas-liquid separator 6 are both connected to the impurity storage tank 10 through pipes and valves; the discharge port of the first condenser 4 is also connected to the ethanol storage tank 11 through a pipe; the water outlet (not marked) at the bottom of the toluene stratification tank 7 is connected to the water storage tank 12 through a pipe and a valve; the brine outlet (not marked) at the bottom of the salt tower 8 is connected to the brine storage tank 13 in sequence through pipes and valves.

[0025] In actual production, the crude toluene in the crude toluene storage tank 1 is transported to the evaporator 2, and the material is first heated to 85°C to distill off the ethanol in the material (boiling point 78.32°C). The ethanol gas passes through the first gas-liquid separator 3 to separate a small amount of impurities and then enters the first condenser 4 to condense into liquid, which is then transported to the ethanol storage tank 11 for temporary storage; after the ethanol separation is completed, the temperature is raised to 120°C (toluene boiling point 110.6°C) to start distilling toluene, and the toluene vapor enters the first gas-liquid separator 3, the first condenser 4, the second condenser 5 and the second gas-liquid separator 6 in sequence to separate the impurities. The remaining impurities and part of the water in the toluene are then transported to the toluene stratification tank 7 for static stratification. The upper layer is toluene containing 2%-3% water. The upper liquid is transported to the salt tower 8 for further dehydration to obtain toluene with a water content of less than 0.05%; if the moisture content in the toluene does not meet the salt tower inlet standard (2%-3%), the water-containing toluene is returned to the toluene stratification tank for further separation of water and toluene, wherein the separated water is collected in the water storage tank, and the unseparated water is sent to the salt tower together with the toluene for further separation. If the toluene content output by the salt tower is higher than the set standard, the toluene is returned to the salt tower for further separation.

[0026] It should be understood that these embodiments are intended only to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the contents of the present invention, those skilled in the art may make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of this application.

Claims

1. A toluene purification device for the production of etilefrine hydrochloride, characterized by: It includes a crude toluene storage tank, an evaporator, and a first gas-liquid separator which are connected in sequence through pipes and valves; the first gas-liquid separator is provided with a light phase discharge port and a heavy phase discharge port, and the light phase discharge port of the first gas-liquid separator is connected in sequence to a first condenser, a second condenser, and a second gas-liquid separator through pipes and valves; the second gas-liquid separator is provided with a light phase discharge port and a heavy phase discharge port, and the light phase discharge port of the second gas-liquid separator is connected to a toluene stratification tank; the toluene outlet at the top of the toluene stratification tank is connected in sequence to a salt tower through pipes and valves, and the toluene outlet at the top of the salt tower is connected in sequence to an anhydrous toluene storage tank through pipes and valves.

2. The toluene purification device in the production of etilefrine hydrochloride according to claim 1, characterized in that: The evaporator is a rising film evaporator, and a pipeline thermometer and a steam regulating valve are provided in the pipeline between the evaporator and the first gas-liquid separator.

3. The toluene purification device in the production of etilefrine hydrochloride according to claim 1, characterized in that: The discharge port of the first condenser is also connected to the ethanol storage tank through a pipeline.

4. The toluene purification device in the production of etilefrine hydrochloride according to claim 1, characterized in that: The first condenser and the second condenser are both spiral plate condensers.

5. The toluene purification device in the production of etilefrine hydrochloride according to claim 1, characterized in that: The heavy phase discharge ports of the first gas-liquid separator and the second gas-liquid separator are both connected to the impurity storage tank through pipelines and valves.

6. The toluene purification device in the production of etilefrine hydrochloride according to claim 1, characterized in that: The water outlet at the bottom of the toluene stratification tank is communicated with a water storage tank through a pipeline and a valve.

7. The toluene purification device in the production of etilefrine hydrochloride according to claim 1, characterized in that: The brine outlet at the bottom of the salt tower is connected to the brine storage tank in sequence through pipelines and valves.

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